title: Full evaporation headspace gas chromatography for sensitive determination of high boiling point volatile organic compounds in low boiling matrices.
abstract: Determination of volatile organic components (VOC's) is often done by static headspace gas chromatography as this technique is very robust and combines easy sample preparation with good selectivity and low detection limits. This technique is used nowadays in different applications which have in common that they have a dirty matrix which would be problematic in direct injection approaches. Headspace by nature favors the most volatile compounds, avoiding the less volatile to reach the injector and column. As a consequence, determination of a high boiling solvent in a lower boiling matrix becomes challenging. Determination of VOCs like: xylenes, cumene, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMA), N-methyl-2-pyrrolidone (NMP), 1,3-dimethyl-2-imidazolidinone (DMI), benzyl alcohol (BA) and anisole in water or water soluble products are an interesting example of the arising problems. In this work, a headspace variant called full evaporation technique is worked out and validated for the mentioned solvents. Detection limits below 0.1 μg/vial are reached with RSD values below 10%. Mean recovery values ranged from 92.5 to 110%. The optimized method was applied to determine residual DMSO in a water based cell culture and DMSO and DMA in tetracycline hydrochloride (a water soluble sample).
authors.affiliation: KU Leuven, Pharmaceutical Analysis, Faculty of Pharmaceutical Sciences, Herestraat 49, O&N2, PB923, B-3000 Leuven, Belgium.
authors.forename: Didi
authors.initials: D
authors.lastname: Mana Kialengila
authors.forename: Kris
authors.initials: K
authors.lastname: Wolfs
authors.forename: John
authors.initials: J
authors.lastname: Bugalama
authors.forename: Ann
authors.initials: A
authors.lastname: Van Schepdael
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D016014:Linear Models; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D044366:Transition Temperature; D055549:Volatile Organic Compounds / Q000032:analysis* / Q000737:chemistry
chemical_list: D055549:Volatile Organic Compounds
keywords: Full evaporation technique; Headspace-gas chromatography; High boiling volatile compounds; Sensitivity